RESEARCH REPORT CONTROLLED BREAKING OF MUMMIFIED …

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RESEARCH REPORT CONTROLLED BREAKING OF MUMMIFIED WOOD FOR USE IN PALEOENVIRONMENTAL ANALYSIS BENJAMIN HOOK* 1 , JOCHEN HALFAR 1 , ZE’EV GEDALOF 2 , and JO ¨ RG BOLLMANN 1 1 Department of Earth Sciences, University of Toronto, Toronto, ON M5S 3B1, Canada 2 Department of Geography, University of Guelph, Guelph, ON N1G 2W1, Canada ABSTRACT The discovery of exceptionally well-preserved Paleogene wood fossils (ca. 55–53 Ma) within Canadian Arctic diamond-bearing kimberlites prompted a paleoclimatic study of the Paleocene-Eocene Transition. The samples are not petrified, but have been ‘‘mummified’’ by their inclusion in pyroclastic debris and still contain primordial wood material. However, preferential cellulose loss has rendered the wood very fragile, precluding the use of standard dendrochronological methods of surface preparation. Similar to archaeological charcoal, breaking the mummified wood allows superior visualization of tree-ring boundaries and wood anatomy, but often produces irregular surfaces making microscopic examination difficult. Therefore, a simple aluminum clamp was constructed to break radial wood transects in a controlled manner for the purpose of collecting dendrochronological and wood-anatomical data for paleoclimatic reconstructions. Because it does not require the use of chemical treatments or stabilizing resins, the wood remains chemically unaltered, allowing chemical and isotopic analyses to be undertaken. Future studies of fragile woods may benefit from this method of controlled breaking if sanding is ineffective. RE ´ SUME ´ La de ´couverte de fossiles bois du Pale ´oge `ne (55–53 Ma), exceptionnellement bien conserve ´s, dans des kimberlites diamantife `res dans l’Arctique canadienne a incite ´a ` une etude pale ´oclimatique de la transition Pale ´oce `ne-Eoce `ne. Les e ´chantillons ne sont pas petrifies. Ils ont e ´te ´ «momifie ´» de par leur inclusion dans des de ´bris pyroclastiques et contiennent toujours du mate ´riel du bois primordial. Toutefois, la perte de cellulose pre ´fe ´rentiel a rendu le bois tre `s fragile, ce qui exclus l’utilisation de me ´thodes dendrochronologiques usuelles afin de preparer la surface. Comme pour les charbons de bois arche ´ologiques, en brisant le bois momifie ´, il est possible de visualiser avec acuite ´ les frontie `res des arbres-anneau et l’anatomie du bois. Cependant, ceci produit souvent des surfaces irre ´gulie `res qui rendant l’examen microscopique difficile. Par conse ´quent, une pince en aluminium simple a e ´te ´ construite afin de briser des transects radiaux de bois de manie `re contro ˆ le ´e, dans le but de recueillir des donne ´es dendrochronologiques et des donne ´es de l’aspect anatomique du bois, afin d’e ´tablir des reconstructions pale ´oclimatiques. Parce que l’utilisation de traitements chimiques ou de re ´sines de stabilisation n’est pas ne ´ccessaire, le fossile de bois reste chimiquement inchange ´, ce qui permet des analyses chimiques et isotopiques. Les e ´tudes futures de bois fragiles peuvent be ´ne ´ficier de notre me ´thode de rupture contro ˆ le ´e si le ponc ¸age est inefficace. Keywords: Paleocene/Eocene transition, non-permineralized fossil wood, fragile wood, surface preparation, automated microscopic scanning, tree-ring measurement, wood anatomy, dendrochro- nology, paleoclimatology. INTRODUCTION ‘‘Mummified’’ woods, which have not been permineralized, are an important paleoclimatic archive. These rare fossils may be found in a *Corresponding author: [email protected] TREE-RING RESEARCH, Vol. 69(2), 2013, pp. 87–92 DOI: http://dx.doi.org/10.3959/1536-1098-69.2.87 Copyright 2013 by The Tree-Ring Society 87

Transcript of RESEARCH REPORT CONTROLLED BREAKING OF MUMMIFIED …

untitledCONTROLLED BREAKING OF MUMMIFIED WOOD FOR USE IN PALEOENVIRONMENTAL ANALYSIS
BENJAMIN HOOK*1, JOCHEN HALFAR1, ZE’EV GEDALOF2, and JORG BOLLMANN1
1Department of Earth Sciences, University of Toronto, Toronto, ON M5S 3B1, Canada
2Department of Geography, University of Guelph, Guelph, ON N1G 2W1, Canada
ABSTRACT
The discovery of exceptionally well-preserved Paleogene wood fossils (ca. 55–53 Ma) within Canadian
Arctic diamond-bearing kimberlites prompted a paleoclimatic study of the Paleocene-Eocene Transition.
The samples are not petrified, but have been ‘‘mummified’’ by their inclusion in pyroclastic debris and still
contain primordial wood material. However, preferential cellulose loss has rendered the wood very fragile,
precluding the use of standard dendrochronological methods of surface preparation. Similar to
archaeological charcoal, breaking the mummified wood allows superior visualization of tree-ring boundaries
and wood anatomy, but often produces irregular surfaces making microscopic examination difficult.
Therefore, a simple aluminum clamp was constructed to break radial wood transects in a controlled manner
for the purpose of collecting dendrochronological and wood-anatomical data for paleoclimatic
reconstructions. Because it does not require the use of chemical treatments or stabilizing resins, the wood
remains chemically unaltered, allowing chemical and isotopic analyses to be undertaken. Future studies of
fragile woods may benefit from this method of controlled breaking if sanding is ineffective.
RESUME
La decouverte de fossiles bois du Paleogene (55–53 Ma), exceptionnellement bien conserves, dans des
kimberlites diamantiferes dans l’Arctique canadienne a incite a une etude paleoclimatique de la transition
Paleocene-Eocene. Les echantillons ne sont pas petrifies. Ils ont ete «momifie» de par leur inclusion dans des
debris pyroclastiques et contiennent toujours du materiel du bois primordial. Toutefois, la perte de cellulose
preferentiel a rendu le bois tres fragile, ce qui exclus l’utilisation de methodes dendrochronologiques usuelles
afin de preparer la surface. Comme pour les charbons de bois archeologiques, en brisant le bois momifie, il
est possible de visualiser avec acuite les frontieres des arbres-anneau et l’anatomie du bois. Cependant, ceci
produit souvent des surfaces irregulieres qui rendant l’examen microscopique difficile. Par consequent, une
pince en aluminium simple a ete construite afin de briser des transects radiaux de bois de maniere controlee,
dans le but de recueillir des donnees dendrochronologiques et des donnees de l’aspect anatomique du bois,
afin d’etablir des reconstructions paleoclimatiques. Parce que l’utilisation de traitements chimiques ou de
resines de stabilisation n’est pas neccessaire, le fossile de bois reste chimiquement inchange, ce qui permet des
analyses chimiques et isotopiques. Les etudes futures de bois fragiles peuvent beneficier de notre methode de
rupture controlee si le poncage est inefficace.
Keywords: Paleocene/Eocene transition, non-permineralized fossil wood, fragile wood, surface
preparation, automated microscopic scanning, tree-ring measurement, wood anatomy, dendrochro-
nology, paleoclimatology.
permineralized, are an important paleoclimatic
archive. These rare fossils may be found in a*Corresponding author: [email protected]
TREE-RING RESEARCH, Vol. 69(2), 2013, pp. 87–92
DOI: http://dx.doi.org/10.3959/1536-1098-69.2.87
et al. 2003), and in tertiary lignite mines (Jahren
and Sternberg 2003; Sahay 2011). Because they
contain primordial wood material, high-resolution
stable isotope studies are possible (Jahren and
Sternberg 2008; Csank et al. 2011a, 2011b).
However, because of preferential cellulose loss,
non-permineralized woods commonly have ex-
tremely low cellulose yields (0–10%) (Jahren and
Schubert pers. comm. 2011) resulting in poor
structural stability. Consequently, the wood cells
are so delicate that any standard preparation tools
(saws, razor blades, sandpaper) applied directly to
the surface destroy them. Therefore, alternate
methods of surface preparation are required for
mummified wood.
vated during operations at two kimberlite mines,
Rio Tinto’s Diavik Diamond Mine (64u299460N,
110u169240W) and BHP Billiton’s Ekati Diamond
Mine (64u429490N, 110u379100W) near Lac de
Gras, Northwest Territories, Canada (Wolfe
et al. 2012). The kimberlites erupted at 55.5 Ma
(Diavik) and 53.6 Ma (Ekati) 60.6 Ma, tempo-
rally near the Paleocene-Eocene Thermal Maxi-
mum and Elmo hyperthermal events, respectively
(Creaser et al. 2004; Heaman et al. 2004; Zachos et
al. 2010). Originating from magmatic dykes,
pyroclastic debris cooled adiabatically to 25–
400uC within hours (Wilson and Head 2007) to
days or months (Sparks et al. 2007) after the
kimberlite eruption. Fragments of wood and shale
xenoliths were instantaneously incorporated up to
.300 m deep into the emplacement crater (Sweet
et al. 2003).
rial, including the oldest stable fossil a-cellulose
found to date, confirmed by Fourier transform
infrared (FTIR) analysis (ANALEST lab, Univer-
sity of Toronto). FTIR absorption peaks of the
fossil a-cellulose match peaks characteristic of
laboratory standard (Sigma-Aldrich) a-cellulose
(900 cm21 and 1375 cm21) (Wolfe et al. 2012). The
exceptional preservation is likely caused by
anaerobic burial in rapidly cooled pyroclastic
debris at the time of kimberlite emplacement.
However, because of the extreme fragile nature of
the material, published surface preparation meth-
ods (e.g. Hall 1939; Krusic and Hornbeck 1989;
Schweingruber 1990; Jones and Rowe 1999;
Angeles 2001; Speer 2010; Donato and Timme
2012) were ineffective for preserving mummified
wood cell structures on long radial transects
suitable for dendrochronological measurements.
features on a transverse surface of radial transects
similar in size to a standard dendrochronological
tree core (ca. 0.5 cm wide, .10 cm long). Some
methods that work well with small samples
(,2 cm3) such as scanning electron microscopy,
or epoxy resin embedding and microsectioning
could not produce surfaces large enough for tree-
ring width measurement (Jones and Rowe 1999).
Moreover, we wished to maintain the chemical
and isotopic integrity of the wood for subsequent
geochemical analyses. Therefore, we tested two
methods for viewing the transverse surface: (1) the
standard method of cutting, mounting and sand-
ing cross-sections, and (2) controlled breaking of
wood transects using a specially-designed breaking
machine.
METHODS
We applied protective media (paraffin or
expanding/hardening foam) to the outer circum-
ference of each dried sample to prevent the outer
tree rings from flaking off during cutting. Then,
we cut cross-sections (ca. 3 cm) from each sample
with a 90-cm finishing saw (Figure 1a). We
mounted the sections on backing boards, sanded
with progressively finer-grit sandpaper (200 to
2,000 grit), and cleaned the surface with pressur-
ized air (Speer 2010).
monly break samples by hand to expose the
transverse plane (Schweingruber 1990; Jones and
Rowe 1999; Schweingruber and Gartner pers.
comm. 2012). However, manual breaking of the
fragile mummified wood was difficult to control
88 HOOK, HALFAR, GEDALOF, and BOLLMANN
and often resulted in irregular and uneven
surfaces. Therefore, we designed a simple machine
for the purpose of breaking wood transects in a
controlled manner to expose the transverse plane
without marring the wood surface. Radial tran-
sects (transversal width: ca. 0.5 cm; radial-longi-
tudinal height: 2–3 cm) were cut from cross-
sections including pith if present. We then sanded
radial surfaces flat, cleaned with compressed air,
applied masking tape to both sides of each
transect to avoid losing wood fragments during
processing, and labeled each transect (Figure 1b).
In some cases it was necessary to reconstruct the
original cross-section from a series of transects
(e.g. if a particular transect was interrupted by an
insect gallery). In such cases it was necessary to
note top, bottom, inner (pith), and outer (bark)
sides of each transect relative to the cross-section
to aid in reassembly.
structed in the academic machine shop at the
University of Toronto at Mississauga from
aluminum for a cost of about $300 (Figure 1c).
It consists of a 200 3 70 3 5 mm ‘‘base-1’’ (n.b. a
45u wedge was removed from the bottom of the
‘‘fulcrum’’ side – see Discussion section for
Figure 1. (a) Cardboard forms were used to keep expanding foam within the desired area while hardening overnight, then cross-
sections (ca. 3 cm) were cut using a fine-toothed saw (scale bar 5 20 cm). (b) Transects were cut perpendicularly to annual tree-ring
boundaries, using masking tape to prevent loss of material during sawing and to enable sample labeling (scale bar 5 10 mm). (c)
Diagram of controlled breaking machine (see Methods section for detailed dimensions of components). Components: I 5 base-1, II
5 backstop, III 5 vice-1, IV 5 vice-2, V 5 base-2, VI 5 fulcrum point (unattached). (d) The controlled breaking machine may be
mounted to a lab desk or bench using two large C-clamps. A prepared mummified wood transect is shown in the device, ready to be
broken (scale bar 5 10 mm).
Controlled Breaking of Mummified Wood 89
details); a 200 3 18 3 25 mm ‘‘backstop’’ bolted
to the base-1, exactly 1 cm from the fulcrum side
(n.b. cylindrical cavities were milled from the
backstop to allow space for the wing nuts); a 200
3 10 3 5 mm ‘‘vice-1’’ attached to the base-1
(fulcrum side) using machine screws and wing
nuts; a 200 3 10 3 5 mm ‘‘base-2’’ (n.b. a
matching 45u wedge was removed from the
fulcrum side); and a 200 3 10 3 5 mm ‘‘vice-2’’
attached to the base-2 also using machine screws
and wing nuts.
controlled breaking machine between the base-1
and the vice-1 and tightened the wing nuts firmly,
but not so tightly as to induce smashing
(Figure 1d). Then we scored both sides of each
transect with a razor blade along the edge of the
vice-1 (through the tape and ca. 1 mm into the
wood), thus guiding the location of the break. We
then attached the base-2 and vice-2 firmly to the
exposed half of each transect, breaking them
manually by pressing downward and inward.
Once broken, we mounted the wood using clay
such that the longitudinal axis was vertical, and
used pressurized air to clean.
We used an automated reflected light micro-
scope (Olympus VS-BX) and geo.TS software
(Olympus Soft Imaging Solutions) to capture digital
scans of the samples at high-resolution (503 to
2003 magnification). This system allows for ex-
tended focal depth, by capturing multiple images of
a 3D surface (maximum XYZ scanning space: 130
3 70 3 6 mm), assembling a 2D photomo-
saic (please visit www.utm.utoronto.ca/,w3halfar/
3D scanning). A flatbed scanner may also be used if
such a 3D scanning system is unavailable; however,
areas of wood that are not flat against the surface of
the scanner will appear slightly blurred in the final
scan. This limitation can be overcome by working
with the actual wood sample in conjunction with the
digital scan during crossdating and measurement.
A reflected light microscope and measure-
ment stage (e.g. Velmex) could be used to collect
linear measurements. However, the mummified
wood tree rings in this study were physically
compacted. Diagenetic compaction of tree rings
was unequally distributed (more common in
earlywood than latewood). Therefore, to collect
tree-ring width data for this study, measurements
were taken along diagenetically deformed ray cell
paths. In modern trees, ray cells are normally
oriented perpendicularly to annual boundaries, so
this is a good approximation of the tree-ring series
before compaction.
sanding method kept cross-sections intact, the
sandpaper abraded the wood cells, blurring the
surface (Figure 2a). Several annual boundaries
were missed altogether that were clearly visible
when using the controlled breaking method
(Figure 2b). Important wood anatomical features
obscured by sanding (Figure 2c) were evident after
breaking, including true annual boundaries, resin
canals, and ‘‘false’’ rings (Figure 2d). Identifica-
tion of such features is crucial for accurate
crossdating and measurement of tree rings and
wood cells, which is critical in our goal of
understanding forest ecological processes and
climates of ancient environments.
depending on the size and condition of samples. In
studies of less-fragile woods, a metal harder than
aluminum may provide more stability during
breaking. Note that the removal of ca. 45u of
aluminum on the bottom ‘‘fulcrum’’ sides of base-
1 and base-2 was essential for proper ‘‘hinging’’ of
the transect during breaking. Without this mod-
ification, mummified wood transects were more
likely to crumble rather than break cleanly
because the hinge point was too low. The fixed
1-cm backstop depth produced samples with a
consistent height, which is helpful when multiple
transects from a cross-section are reassembled.
Also, note that applying electrical tape to the
‘‘inner’’ surfaces of both bases and vices helped
grip transects during breaking. To avoid uneven
breaking, it was important to make sure the radial
surfaces of transects were cut parallel and sanded
flat. Additional small (2 cm) C-clamps may be
placed along the base-2 and vice-2 to help
90 HOOK, HALFAR, GEDALOF, and BOLLMANN
distribute the force evenly along longer transects,
and aid in breaking uniformly.
The unique diagenesis and preservation of
mummified wood in kimberlite rock requires
alternate methods of surface preparation. The
samples may be quite large (.60 cm diameter), but
compositionally similar to charcoal because of
their rapid entombment in pyroclastic debris. This
burial environment is very different from that of
most archaeological charcoals, which are usually
found as small fragments (,2 cm) because of
taphonomic forces. The method of controlled
breaking introduced here allows clear visualization
of non-permineralized fossil wood, enabling pre-
cise determination of annual tree-ring boundaries
along continuous transects, similar to a tree core.
This minimally invasive approach leaves the
sample unaltered by chemical additives so that
subsequent analyses may be conducted. Future
studies of fragile wood fossils may benefit from
this method of controlled breaking.
ACKNOWLEDGMENTS
The authors would like to thank Diavik
Diamond Mine Inc. (DDMI - Rio Tinto) and
Figure 2. (a) Digital scan of mummified wood after sanding method (scale bar 5 1 mm). (b) Digital scan of same sample as in (a)
after controlled breaking method. Two transects have been reassembled into their original sequence after being cut and scored with
a razor blade (scale bar 5 1 mm). (c) Scanning electron microscope (SEM) image of sample after sanding method (scale bar 5
0.1 mm). (d) SEM image of the same sample as in (c) after controlled breaking method (scale bar 5 0.1 mm). Detailed wood-
anatomical features were apparent in the broken sample (d) which were not visible in the sanded sample (c), including annual
boundaries (white arrows), false rings (black arrows), diagenetically crushed earlywood (above white arrows), and resin canals
(bottom of c and d).
Controlled Breaking of Mummified Wood 91
Ekati Diamond Mine (BHP Billiton) for generous
access to the mummified wood, especially David
Eichenberg, Hayley McLean, Gus Fomradas, and
Yuri Kinakin at DDMI for a tour of Diavik Mine;
Peter Duggan (Academic Machine Shop, Univer-
sity of Toronto at Mississauga) for construction of
the controlled breaking machine; Marie Puddister
(Department of Geography, University of Guelph)
for drafting Figure 1c; Hope Jahren and Brian
Schubert for discussions about mummified wood
cellulose extractions (American Geophysical
wood preparation techniques (International Course
on Wood Anatomy, Klosters-Dorf, Switzerland,
2012); Monique Mailloux for assistance with
French translation; and two anonymous reviewers
whose comments helped to improve the clarity and
organization of this manuscript.
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92 HOOK, HALFAR, GEDALOF, and BOLLMANN
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/ENU (Settings for the Rampage workflow.) >> >> setdistillerparams << /HWResolution [2400 2400] /PageSize [612.000 792.000] >> setpagedevice